注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留

doi:10.13305/j.cnki.jts.20210804.001

茶叶科学 ›› 2021, Vol. 41 ›› Issue (5): 717-730.doi: 10.13305/j.cnki.jts.20210804.001

注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留

马佳丽^1,2,3,4, 王晨^1,3,4,*, 陈红平^1,3,4, 柴云峰^1,3,4, 诸力^1,3,4, 刘新^1,3,4,*

1.中国农业科学院茶叶研究所,浙江杭州 310008;
2.中国农业科学院研究生院,北京 100081;
3.农业农村部茶叶质量安全控制重点实验室,浙江杭州 310008;
4.农业农村部茶叶产品质量安全风险评估实验室（杭州）,浙江杭州 310008

收稿日期:2021-02-01 修回日期:2021-03-01 出版日期:2021-10-15 发布日期:2021-10-12
通讯作者: *wangchen@tricaas.com;liuxin@tricaas.com
作者简介:马佳丽,女,硕士研究生,主要从事茶叶质量安全研究。
基金资助:
财政部和农业农村部：国家现代农业产业技术体系（CARS-19）、中国农业科学院创新团队（CAAS-ASTIP-2014-TRICAAS-06）、国家农产品质量安全风险评估项目（GJFP2020001）

Rapid Determination of 24 Pesticide Residues in Tea by in-Syringe Dispersive Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

MA Jiali^1,2,3,4, WANG Chen^1,3,4,*, CHEN Hongping^1,3,4, CHAI Yunfeng^1,3,4, ZHU Li^1,3,4, LIU Xin^1,3,4,*

1. Tea Research Institute, Chinese Academy of Agriculture Sciences, Hangzhou 310008, China;
2. Graduate School, Chinese Academy of Agriculture Sciences, Beijing 100081, China;
3. Key Laboratory of Tea Quality and Safety Control, Ministry of Agriculture and Rural Affairs, Hangzhou 310008, China;
4. Laboratory of Quality and Safety Risk Assessment for Tea Products (Hangzhou), Ministry of Agriculture and Rural Affairs, Hangzhou 310008, China

Received:2021-02-01 Revised:2021-03-01 Online:2021-10-15 Published:2021-10-12

摘要/Abstract

摘要： 基于茶叶基质特点,开发了注射器内分散固相萃取快速前处理技术,建立了茶叶中24种农药残留超高效液相色谱-串联质谱检测方法。茶叶样品经乙腈提取,无水MgSO₄盐析,在设计的注射器装置内以N-丙基乙二胺键合硅胶和石墨化炭黑作为分散吸附剂进行净化,超高效液相色谱-串联质谱法进行检测。在3个添加水平（0.01、0.05、0.5βmg·kg^-1）下,红茶和绿茶中24种农药的平均回收率为61.7%~98.8%,相对标准偏差为0.4%~5.5%,准确度和精密度良好。24种农药的红茶和绿茶基质标准工作液线性关系良好,相关系数（R²）均大于0.995,检出限（LOD）和定量限（LOQ）分别为0.05~5.36βμg·kg^-1和0.18~17.86βμg·kg^-1,该方法具有良好的灵敏度。本方法具有简便快捷、所需仪器少、省时等优势,适用于茶叶中多农药残留的定量检测。

关键词: 茶叶, 超高效液相色谱-串联质谱, 农药残留, 注射器内分散固相萃取

Abstract: Based on the characteristics of tea matrix, a rapid pretreatment technology of in-syringe dispersive solid phase extraction (dSPE) was developed, and an analytical method based on ultra high performance liquid chromatography-tandem mass spectrometry was established for the detection of 24 pesticide residues in tea. Tea samples were extracted using acetonitrile, salted-out with MgSO₄, purified with primary secondary amine and graphitized carbon black as dispersive adsorbents in designed syringe devices, and detected by UPLC-MS/MS. Recoveries of 24 pesticides in black and green teas were 61.7%-98.8% at three spiked levels (0.01βmg·kg^-1, 0.05βmg·kg^-1 and 0.5βmg·kg^-1), which indicated high accuracy with the relative standard deviations of 0.4%-5.5%. The calibration curves of 24 pesticides in black and green teas showed good linearity with correlation coefficients (R²) higher than 0.995. The limits of detection (LOD) and the limits of quantitation (LOQ) were 0.05-5.36βμg·kg^-1 and 0.18-17.86βμg·kg^-1, respectively, which show high sensitivity of this method. Being simple, fast, less instrument required and time-saving, this method is suitable for quantification of multiple pesticide residues in tea.

Key words: tea, ultra high performance liquid chromatography-tandem mass spectrometry, pesticide residues, in-syringe dispersive solid phase extraction

中图分类号:

马佳丽, 王晨, 陈红平, 柴云峰, 诸力, 刘新. 注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留[J]. 茶叶科学, 2021, 41(5): 717-730. doi: 10.13305/j.cnki.jts.20210804.001.

MA Jiali, WANG Chen, CHEN Hongping, CHAI Yunfeng, ZHU Li, LIU Xin. Rapid Determination of 24 Pesticide Residues in Tea by in-Syringe Dispersive Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Tea Science, 2021, 41(5): 717-730. doi: 10.13305/j.cnki.jts.20210804.001.

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注射器内分散固相萃取-超高效液相色谱-串联质谱法快速测定茶叶中24种农药残留

Rapid Determination of 24 Pesticide Residues in Tea by in-Syringe Dispersive Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

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